# US 5,691,445 A · Devolatilization > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,691,445 A - Document ID: US5691445A - Status: Granted - Kind: A - Application number: 08/623,228 - Filed: 1996-03-28 - Granted: 1997-11-25 - Earliest claimed: 1996-03-28 - Assignees: Novacor Chemicals (International) S.A. - Inventors: Steven M. Krupinski; James T. McQueen - Web page: https://patentgrep.com/patent/US5691445A ## CPC - C08F 6/28: Purification - C08F 6/001: {Removal of residual monomers by physical means} - C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS ## Abstract A polymer melt may be devolatilized to less than 500, preferably less than 150 ppm of residual volatile material by injecting into the melt an amount of a super critical fluid greater than the amount of residual volatile material in the melt, typically not more than about 10 weight %, and passing the melt through a flash chamber devolatilizer at a pressure of 12 mm of Hg or less at a temperature of from 200.degree. to 350.degree. C. ## Claims ### Claim 1 A process for reducing the amount of residual monomer, and solvent to less than 300 parts per million in a polymer or polymer blend containing less than 5 weight % of such residual monomer, and solvent which process comprises: (i) heating and maintaining said polymer or polymer blend as a melt at a temperature from 200.degree.-270.degree. C.; (ii) injecting into said melt an amount of a non-oxidizing super critical fluid greater than the amount of residual monomer, and solvent but less than 5 weight %, said injection being at temperatures of from 200.degree. to 270.degree. C. and pressures to dissolve the super critical fluid in said melt; and (iii) maintaining said melt at a temperature from 200.degree.-270.degree. C. while exposing said polymer to a pressure maintained at less than 8 Torr. ### Claim 2 (depends on 1) The process according to claim 1 wherein said polymer or polymer blend contains less than 2% of residual monomer and solvent. ### Claim 3 (depends on 2) The process according to claim 2 wherein said super critical fluid is injected into said polymer or polymer blend at a pressure from 1,000 to 15,000 psig. ### Claim 4 (depends on 3) The process according to claim 3 wherein said super critical fluid is selected from the group consisting of CO.sub.2, C.sub.4-6 alkanes and nitrogen. ### Claim 5 (depends on 4) The process according to claim 4, wherein said polymer or polymer blend is selected from the group consisting of: (A) polymers comprising: (i) from 100 to 30 weight % of one or more monomers selected from the group consisting of C.sub.8-12 vinyl aromatic monomers which are unsubstituted or substituted by a C.sub.1-4 alkyl radical; and (ii) from 0 to 70 weight % of one or more monomers selected from the group consisting of C.sub.1-4 alkyl esters of acrylic or methacrylic acid, acrylonitrile and methacrylonitrile; which polymers may be grafted on to from 0 to 40 weigh % of one or more rubbery polymers selected from the group consisting of: (iii) polymers consisting essentially of one or more C.sub.4-6 conjugated diolefin monomers; and (iv) polymers consisting essentially of from 20 to 80 weight % of one or more C.sub.8-12 vinyl aromatic monomers and from 80 to 20 weight % of one or more C.sub.4-6 conjugated diolefins; (B) polymers comprising: (i) from 95 to 85 weight % of one or more C.sub.8-12 vinyl aromatic monomers; and (ii) from 15 to 5 weight % of maleic anhydride; (C) a blend of said polymers and polyphenylene oxide; (D) polyamides; and (E) aromatic polyesters. ### Claim 6 (depends on 5) The process according to claim 5 wherein said polymer or polymer melt is maintained at a temperature from 225.degree. to 235.degree. C. ### Claim 7 (depends on 6) The process according to claim 6 wherein said super critical fluid is nitrogen and is injected at pressures from 10,000 to 15,000 psig. ### Claim 8 (depends on 6) The process according to claim 6, wherein said super critical fluid is CO.sub.2 and is injected at pressures from 1,000 to 5,000 psig. ### Claim 9 (depends on 7) The process according to claim 7, wherein said melt is passed through an extruder having vacuum ports. ### Claim 10 (depends on 9) The process according to claim 9, wherein said pressure is less than 5 Torr. ### Claim 11 (depends on 8) The process according to claim 8, wherein said melt is passed through an extruder having vacuum ports. ### Claim 12 (depends on 11) The process according to claim 11, wherein said pressure is less than 5 Torr. ### Claim 13 (depends on 7) The process according to claim 7, wherein said melt is passed through a flash chamber. ### Claim 14 (depends on 13) The process according to claim 13, wherein the pressure is less than 5 Torr. ### Claim 15 (depends on 8) The process according to claim 8, wherein said melt is passed through a flash chamber. ### Claim 16 (depends on 15) The process according to claim 15, wherein said pressure is less than 5 Torr. ### Claim 17 (depends on 10) The process according to claim 10, further including adding to said melt from 1,000 to 2,500 parts per million of a nucleating agent. ### Claim 18 (depends on 12) The process according to claim 12, further including adding to said melt from 1,000 to 2,500 parts per million of a nucleating agent. ### Claim 19 (depends on 14) The process according to claim 14, further including adding to said melt from 1,000 to 2,500 parts per million of a nucleating agent. ### Claim 20 (depends on 16) The process according to claim 16, further including adding to said melt from 1,000 to 2,500 parts per million of a nucleating agent. ### Claim 21 (depends on 16) The process according to claim 16 further comprising depositing said polymer or polymer blend on one or more distributor trays within said flash chamber. ### Claim 22 (depends on 16) The process according to claim 16 wherein the inlet line into said flash chamber has a pressure restriction device or head. ### Claim 23 (depends on 16) The process according to claim 16 wherein said polymer or polymer blend is selected from the group consisting of polystyrene, HIPS, SAN, ABS, SMA and copolymers of styrene and methyl methacrylate.